In this project, we used high resolution magic angle spinning (HRMAS) 'HMRS, a spectroscopic method that is rapid and requires only small amounts of unprocessed tissue samples, to assess neuronal damage using multiple tissue samples from differently affected brain regions in a case of Pick disease, a human neurodegenerative disorder. Unlike chemical extraction or other forms of tissue processing, this new method analyzes tissue directly, thus minimizing artifacts. In this study, we found an excellent correlation between neuronal loss shown by traditional neurohistopathology and decrease of the neuronal marker N-acetylaspartate (NAA) measured by HRMAS 'HMRS. This result demonstrates for the first time a direct, quantitative link between a decrease in NAA and neuronal loss in a human neurodegenerative disease. As a quantitative method, HRMAS 'HMRS has potential applications in experimental and clinical neuropathologic investigations. It should also provide a rational basis for the interpretation of in vivo 'HMRS studies of human neurological disorders.